WO2014025872A1 - Process for starch liquefaction - Google Patents
Process for starch liquefaction Download PDFInfo
- Publication number
- WO2014025872A1 WO2014025872A1 PCT/US2013/053929 US2013053929W WO2014025872A1 WO 2014025872 A1 WO2014025872 A1 WO 2014025872A1 US 2013053929 W US2013053929 W US 2013053929W WO 2014025872 A1 WO2014025872 A1 WO 2014025872A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- starch
- liquefaction
- slurry
- dry substance
- starch slurry
- Prior art date
Links
- 229920002472 Starch Polymers 0.000 title claims abstract description 238
- 235000019698 starch Nutrition 0.000 title claims abstract description 234
- 239000008107 starch Substances 0.000 title claims abstract description 228
- 238000000034 method Methods 0.000 title claims abstract description 69
- 239000002002 slurry Substances 0.000 claims abstract description 99
- 239000000126 substance Substances 0.000 claims abstract description 60
- 108090000790 Enzymes Proteins 0.000 claims description 36
- 102000004190 Enzymes Human genes 0.000 claims description 36
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 17
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 17
- 239000008121 dextrose Substances 0.000 claims description 15
- 230000000593 degrading effect Effects 0.000 claims description 13
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 10
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 10
- 239000004382 Amylase Substances 0.000 claims description 6
- 229920002774 Maltodextrin Polymers 0.000 claims description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 2
- 238000010924 continuous production Methods 0.000 abstract description 2
- 229940088598 enzyme Drugs 0.000 description 33
- 238000010438 heat treatment Methods 0.000 description 17
- 229920002245 Dextrose equivalent Polymers 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000010793 Steam injection (oil industry) Methods 0.000 description 7
- 235000020357 syrup Nutrition 0.000 description 7
- 239000006188 syrup Substances 0.000 description 7
- 230000002255 enzymatic effect Effects 0.000 description 6
- 229920000856 Amylose Polymers 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229940100445 wheat starch Drugs 0.000 description 4
- 108010073178 Glucan 1,4-alpha-Glucosidase Proteins 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000010923 batch production Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 108010065511 Amylases Proteins 0.000 description 2
- 102000013142 Amylases Human genes 0.000 description 2
- 102100022624 Glucoamylase Human genes 0.000 description 2
- 229920000881 Modified starch Polymers 0.000 description 2
- 239000004368 Modified starch Substances 0.000 description 2
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 235000019418 amylase Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 235000019426 modified starch Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 240000001592 Amaranthus caudatus Species 0.000 description 1
- 235000009328 Amaranthus caudatus Nutrition 0.000 description 1
- 235000005273 Canna coccinea Nutrition 0.000 description 1
- 240000008555 Canna flaccida Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- 240000005979 Hordeum vulgare Species 0.000 description 1
- 235000007340 Hordeum vulgare Nutrition 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- 244000151018 Maranta arundinacea Species 0.000 description 1
- 235000010804 Maranta arundinacea Nutrition 0.000 description 1
- 240000008790 Musa x paradisiaca Species 0.000 description 1
- 235000018290 Musa x paradisiaca Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000004713 Pisum sativum Species 0.000 description 1
- 235000010582 Pisum sativum Nutrition 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 240000006394 Sorghum bicolor Species 0.000 description 1
- 235000011684 Sorghum saccharatum Nutrition 0.000 description 1
- 235000012419 Thalia geniculata Nutrition 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 108090000637 alpha-Amylases Proteins 0.000 description 1
- 235000012735 amaranth Nutrition 0.000 description 1
- 239000004178 amaranth Substances 0.000 description 1
- 229940025131 amylases Drugs 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 108010019077 beta-Amylase Proteins 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007071 enzymatic hydrolysis Effects 0.000 description 1
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000013808 oxidized starch Nutrition 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/08—Concentration of starch suspensions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
- C08B30/14—Cold water dispersible or pregelatinised starch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
- C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
- C08B30/18—Dextrin, e.g. yellow canari, white dextrin, amylodextrin or maltodextrin; Methods of depolymerisation, e.g. by irradiation or mechanically
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/02—Monosaccharides
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/22—Preparation of compounds containing saccharide radicals produced by the action of a beta-amylase, e.g. maltose
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K1/00—Glucose; Glucose-containing syrups
- C13K1/06—Glucose; Glucose-containing syrups obtained by saccharification of starch or raw materials containing starch
Definitions
- the present invention relates to a process for the liquefaction of starch present in a starch slurry comprising degraded starch and having a DE of from 0.05 to 9.
- the invention relates to a process for the liquefaction of starch present in a starch slurry comprising degraded starch, said starch slurry having a high dry substance.
- the invention relates to a continuous process for liquefaction of starch present in a starch slurry comprising degraded starch and having a high dry substance.
- Native starch i.e. starch recovered in its original form by extraction from any starch-bearing material, is a starting material for numerous valuable products.
- Starch hydrolysis process can yield glucose syrups, high maltose syrups, very high maltose syrups and the like. From these syrups, several products can be obtained such as crystalline dextrose, polyols and the like.
- the process to hydrolyse starch typically comprises liquefaction and saccharification of native starch in the form of a starch slurry.
- Starch is a natural ingredient with a typical behaviour when it is put into suspension (starch slurry). Above a certain dry substance, the slurry is very difficult to treat and can be responsible for blocking processing equipment. Therefore in current processes, starch slurry to be liquefied typically has a dry substance up to 40 weight/weight % (w/w %) and preferably of from 30 to 35 w/w%, Taking into account heating via steam injection for the liquefaction and subsequent flashing for the saccharifi cation, the Iiquefact thus produced also has a comparable dry substance.
- At least one additional concentration step is necessary to bring the dry substance content of the produced glucose syrups to the desired value, such as for example 60 w/w%, 70 w/w%, 80 w/w%, 85 w/w%, etc.
- This concentration step usually requires a high energy input and is therefore not cost efficient and not environmentally friendly. In the effort to reduce energy consumption of industrial processes, there is a need to provide a more efficient process with significant lower energy consumption.
- EP 0806434A1 describes a batch process for preparing enzyme converted starches.
- US 4,235,965 describes a batch process to hydrolyse starch, starting from a starch slurry having a dry substance of up to 40 w/w%.
- the process is a non-continuous batch process and requires very high amounts of enzymes, consequently the process is relatively inefficient and very costly.
- the present invention relates to a process for the liquefaction of starch present in a starch slurry, wherein said starch slurry has a DE of from 0.05 to 9 and comprises degraded starch.
- the present invention relates to a process for the liquefaction of starch present in a starch slurry, wherein said starch slurry has a DE of from 0.05 to 9 and comprises degraded starch.
- Conventional starch hydrolysis processes typically comprise a liquefaction step followed by a saccharification step
- the starch slurry entering the liquefaction step has a dry substance of up to 40 weight/weight % (w/w%).
- the starch slurry is the starch comprises native starch.
- starch sluixy consists essentially of native starch, For this reason, the dry substance of the starch sluixy is kept at a value of maximum 40 w/w%, typically of from 30 w/w% to 35 w/w%.
- Liquefaction is done at high temperatures, by direct heating to 80 to 160°C, preferably to 90 to around 1 10°C through steam injection, wherein said steam has a pressure of from 9 to 12 bar.
- the starch gelatinizes and viscosity increases.
- heat by steam injection i.e. direct heating, which results in a very fast heating of the starch sluixy and which limits the increase in viscosity and allows a good starch liquefaction.
- heating would be done by indirect heating, the starch would have time to gelatinize and the viscosity increase would be too important and would render pumping and further processing very complicated.
- the starch present in the starch sluixy is broken down into dextrose oligomers, typically through the action of enzymes.
- the liquefied starch sluixy (the liquefact) is saccharified, typically through the action of saccharification enzymes, to yield dextrose containing liquors, maltose containing liquors and the like.
- the botanical origin of the starch is not restricted.
- Suitable sources of starch for use in the present invention are corn, pea, potato, sweet potato, sorghum, banana, barley, wheat, rice, sago, amaranth, tapioca, arrowroot, canna, and low amylose (containing no more that about 10% by weight amylose, preferably no more than 5% by weight amylose) or high amylose (containing at least about 40% by weight amylose) varieties thereof.
- low amylose containing no more that about 10% by weight amylose, preferably no more than 5% by weight amylose
- high amylose containing at least about 40% by weight amylose
- starch is derived from cereals, more preferably from wheat and/or corn.
- starch used as such means for the purpose of the present invention native starch. It is well known in the art how to extract native starch from above mentioned plants. It does not however exclude in any of the process steps of the present invention that modified starch can be added.
- Modified starch refers to starch chemically modified, enzymatically modified, modified by heat treatment or by physical treatment.
- chemically modified includes, but is not limited to crosslinking, modification with blocking groups to inhibit retrogradation, modification by the addition of lipophilic groups, acetylated starches, hydroxyethylated and hydroxypropylated starches, inorganically esterified starches, cationic, anionic and oxidized starches, zwitterionic starches, starches modified by enzymes and combinations thereof.
- Heat treatment includes for example pregelatinization.
- the starch slurry entering the liquefaction step already comprises degraded starch.
- degraded starch results from acid and/or enzymatic hydrolysis of starch and can be one or more of maltodextrins, dextrose, dextrose oligomers, maltose and the like, such products being soluble in water.
- the starch slurry entering the liquefaction step can be obtained by a process comprising:
- said second starch slurry is the starch slurry which will be sent to the liquefaction step.
- the first starch slurry can prepared for example by mixing native starch with water to obtain a slurry having a dry substance of from 25 w/w% to 45 w/w%, preferably 30 w/w% to 45 w/w%, more preferably 35 w/w% to 45 w/w% even more preferably 40 w/w% to 45 w/w%, yet even more preferably above 40 w/w% to 45 w/w%.
- the starch can be in dry powder form or in the form of a slurry.
- the starch can have a dry substance of from 40 w/w% to 90 w/w%.
- the starch is native starch having a dry substance of from 80 w/w% to 90w/w%.
- the pre-liquefact is in fact the first starch slurry which now comprises degraded starch, either because degraded starch has been added to the first starch slurry, or because part of the native starch of the first starch slurry has been degraded.
- the pre-liquefact has a DE (Dextrose Equivalent) of about 0.05 to about 9, preferably of from 0.05 to 8, preferably of from 0.05 to 7, more preferably of from 0.05 to 6, even more preferably of from 1 to 5.
- the DE can be measured with Lane Eynon official method.
- the pre-liquefact has a solubility level of at least 3, preferably at least 6, more preferably of at least 10, even more preferably of at least 20.
- the solubility level is an indication of the amount of starch that is degraded thus solubilized.
- the solubility level of the pre-liquefact is measured according to test A as described in the measurement methods section of this description.
- the pre-liquefact has a similar dry substance as the first starch slurry, i.e. from 25 w/w% to 45 w/w%, preferably 30 w/w% to 45 w/w%, more preferably 35 w/w% to 45 w/w% even more preferably 40 w/w% to 45 w/w%, yet even more preferably above 40 w/w% to 45 w/w%.
- Pre-liquefaction of the first starch slurry to obtain a pre-liquefact can be done by adding degraded starch, as defined above, to the first starch slurry.
- Said degraded starch can be either in powder form and/or in the form of a solution.
- providing a first starch slurry and pre-liquefying the first starch slurry can also be done in one single step, by mixing degraded starch with native starch and water.
- the degraded starch can be in powder form and/or in the form of a solution and the native starch can be in powder form and/or in the form of a slurry.
- degraded starch is produced 'in situ' by acid and/or enzymatic pre- liquefaction of the first starch slurry.
- the pre-liquefaction comprises an enzymatic treatment at a temperature of from 20 to 85°C, typically said temperature is below or maximum 10 °C above the gelatinization temperature of the native starch used to prepare the first starch slurry.
- Enzymatic pre-liquefaction comprises adding one or more starch degrading enzymes to the first starch slurry.
- the one or more enzymes can be for example an a-amylase, a ⁇ -amylase, a glucoamylase, a pullulanase or a combination of these.
- the quantity of enzyme to be added will easily be determined by the person skilled in the art, such as to obtain a pre- liquefact, having a DE of from 0.05 to 9.
- Enzymatic pre-liquefaction is preferably done at a temperature of from 20°C to
- the first starch sluixy can have an initial temperature of from 40°C to 50°C.
- the first starch slurry is first brought to a pH value optimal for the enzyme or enzyme cocktail used.
- a pH value optimal for the enzyme or enzyme cocktail used.
- a pH of from 5 to 6.5 is used for common a- amylases.
- the pH can be modified with any suitable method known in the art, for example by the addition of acid or base depending on whether the initial pH is lower or higher than the desired pH value. The skilled person will easily know how to adapt the pH of the first starch slurry.
- the pre-liquefaction is preferably done in a reactor.
- a reactor Any type of suitable reactor can be used such as for example a tank, plug flow reactor, and the like, with or without agitator, with or without prop flow.
- a closed reactor having one or more inlets and one or more outlets can be used.
- the one or more inlets and the one or more outlets can be situated on the upper and/or lower side of the reactor. Both inlet and outlet are such that the inflow and the outflow of the reactor can be regulated easily manually or automatically.
- the first starch slurry is converted into a starch slurry comprising degraded starch, thus the pre-liquefact, as defined above.
- the pre-liquefact can be sent to the liquefaction step as follows: part of the pre- liquefact is removed from the reactor and sent towards a liquefaction step and the removed part is replaced with starch, preferably native starch, to maintain the slurry in the reactor at a dry substance of from 25 w/w % to 45 w/w%, preferably 30 w/w% to 45 w/w%, more preferably 35 w/w% to 45 w/w% even more preferably 40 w/w% to 45 w/w%, yet even more preferably above 40 w/w% to 45 w/w%; or to increase its dry substance to up to 80w/w%.
- starch preferably native starch
- an additional step can be performed.
- this additional step can comprise the addition of an enzyme and adjusting temperature and/or pH if required.
- the step of removing part of the liquefact and sending it towards a liquefaction step and replacing the removed part with starch or with starch and enzyme is done simultaneously, at the same rate and preferably continuously, without substantial interruption during the process.
- the process can start running in a continuous way.
- continuous means without substantial interruption during the process time.
- Said process time can be from 5 minutes to multiple hours.
- starch can be added to it, in order to increase its dry substance to a value of from 30 w/w% to 80w/w%.
- starch comprises native starch, more preferably starch consists of native starch.
- Starch can also be added simultaneously with the one or more pre-liquefaction enzymes.
- the process of the present invention is further preferably characterized in that it comprises the steps of: a. Providing in a reactor a pre-liquefact at a dry substance of from 25 w/w% to 45 w/w%; and
- step b. and/or step c. one or more starch degrading enzymes can also be added.
- the starch and the one or more starch degrading enzymes in step b. and/or step c. can be mixed together prior to addition or they can be added separately, simultaneously or in sequence. Further, they can be added in several steps or continuously. Preferably, they are added simultaneously, continuously, i.e. without substantial interruption from the start of addition to the end of addition, without prior mixing.
- the present invention relates to a process for the liquefaction of starch present in a starch slurry characterized in that said starch slurry
- degraded starch material obtained by pre-liquefaction of a first starch slurry, said pre-liquefaction comprising enzymatic treatment at a temperature of from 20 and 85°C, and
- - has a dry substance of from 30 w/w% to 80 w/w%.
- the second starch slurry i.e. the starch slurry to be liquefied, can have a dry substance of from 30 w/w% up to 80 w/w%, preferably of from 35 w/w% to 80 w/w %.
- the second starch slurry has a high dry substance: from 40 w/w% to 80 w/w %, more preferably above 40 to 70 w/w %, even more preferably from 45 w/w% to 60 w/w %, yet even more preferably of from 45 w/w% to 55 w/w%, and yet even more preferably of from 48 w/w% to 52 w/w% or from 50 w/w% to 55 w/w %. Due to the presence of the degraded starch, the dry substance of the second starch slurry can be higher than in conventional processes where only native starch is used, without facing the process limitations described earlier.
- one or more starch degrading enzymes are also added in step b. and or step c.
- enzyme with optimal working conditions at pH 3.5 to 6.5 is chosen.
- the quantity of enzyme to be added will easily be determined by the person skilled in the art, and should be such as to maintain the DE of the starch slurry in the reactor at a value of from 0.05 to 9.
- the one or more starch degrading enzymes are thermostable, such as to resist the heating step in a subsequent liquefaction step.
- the starch and the one or more starch degrading enzymes can be mixed together prior to addition or they can be added separately, simultaneously or in sequence. Further, they can be added in several steps or continuously. Preferably, they are added simultaneously, continuously, i.e. without substantial interruption from the start of addition to the end of addition, without prior mixing.
- the temperature in the reactor is maintained at a value of from 20 to 85°C, preferably more preferably from 25 to 75°C, even more preferably from 30 to 70°C and even more preferably from 35 to 60°C.
- the temperature can be maintained by any method known in the art such as by the use of a double jacketed reactor having water circulating at the right temperature, such as to maintain the content of the reactor at the desired temperature.
- the second starch slurry in the reactor is mixed.
- Mixing can be achieved with any suitable method known in the art, such as with a static mixer for example.
- the pH of the second starch sluny depends on the one or more starch degrading enzyme that is used. The person skilled in the art will easily know which pH should be obtained depending on the enzyme used. Preferably, an enzyme with optimal working conditions at pH 3.5 to 6.5 is chosen.
- the viscosity of the second starch sluny is lower than the viscosity of a starch sluny comprising essentially native starch at the same dry substance, temperature and pH. This viscosity lowering effect allows processing a starch slurry having a higher dry substance, compared to conventional liquefaction processes, as explained above.
- Part of the second starch slurry is removed from the reactor via an outlet of the reactor and is sent towards a liquefaction step. The removed part is replaced by starch or by starch and starch degrading enzyme (replacing material), in order to maintain the dry substance of the second starch slurry at a value of from 30 w/w% to 80 w/w%.
- removing and replacing is done at such a rate as to obtain an average retention time of the second starch slurry in the reactor of from 5 minutes to 5 hours, preferably from 30 minutes to 3 hours, more preferably form 2 hour to 3 hours.
- removing and replacing of the second starch slurry is done simultaneously.
- the amount of second starch slurry that is removed is equal to the amount of replacing material that is added, such that the dry substance of the second starch slurry in the reactor does not vary, but is maintained at a same value which is, as explained above, from 30 w/w% to 80 w/w%.
- the step of removing part of the second starch slurry and sending it towards a liquefaction step and replacing the removed part with starch or with starch and enzyme is done continuously, without substantial interruption during the process.
- the process is running in a continuous way.
- starch or starch and enzymes are continuously added into the reactor and part of the second starch slurry is continuously sent to liquefaction, thus step c. of the process is repeated.
- continuous means without substantial interruption during the process time. Said process time can be from 5 minutes to multiple hours.
- an additional step can be performed before the liquefaction step.
- this additional step can comprise the addition of an enzyme and adjusting temperature and/or pH if required.
- Liquefaction is a well-known process in the starch industry and the liquefaction conditions (time, temperature and the like) will be apparent to the person skilled in the art.
- the second starch slurry is typically brought to a temperature of from 90 to 255°C, preferably of from 90 to 150°C, more preferably of from 90 to 130°C, even more preferably of from 90 to 110°C.
- Heating can be done by direct steam injection in a jet cooker. Surprisingly, with the process of the present invention, heating can also be done by indirect heating.
- Liquefaction by steam injection has the disadvantage of adding water in the starch slurry.
- the process of the present invention is further characterized in that the liquefaction stepis done by indirect heating of the second starch slurry at temperature of from 90 to 255°C, preferably from 90 to 150°C, more preferably from 90 to 130°C, even more preferably from 90 to 110°C.
- saccharification can be done.
- the liquefied starch is broken down into dextrose through the action of saccharification enzymes, such as glucoamylase or amyloglucosidase.
- saccharification enzymes such as glucoamylase or amyloglucosidase.
- a high dextrose containing liquor is obtained, having a dry substance similar to or somewhat higher (due to chemical gain) than that of the second starch slurry, i.e. a dry substance of from 40 w/w% to 80 w/w%.
- the dextrose containing liquor obtained by the process of the present invention has a much higher dry substance than dextrose containing liquors obtained by conventional starch hydrolysis processes.
- dextrose can be recovered in the form of crystalline dextrose through crystallisation for example.
- an isomerisation of dextrose can be done to yield fructose.
- a saccharification to maltose can be done.
- a maltose containing liquor is obtained which has a much higher dry substance compared to that of maltose liquors obtained by conventional processes.
- the maltose containing liquor has a dry substance similar to or somewhat higher (due to chemical gain) than that of the second starch slurry, i.e. a dry substance of from 40 w/w% to 80 w/w%. Also here, fewer to no evaporation steps may be required.
- any other suitable treatment can be done after the liquefaction step.
- the present invention relates to a process comprising:
- Test A measurement of solubility level of a starch slurry comprising degraded starch.
- 100 ml of starch slurry comprising degraded starch at about 40°C is filtered through a Macherey- Nagel (MN) 614 1 ⁇ 4 150 mm diameter folded paper filter.
- MN Macherey- Nagel
- the refractive index of the filtrate at 20°C is measured with a refractometer ATAGO DR-A1.
- the refractometer derives the °Brix value from the refractive index and this °Brix corresponds to the solubility level.
- Example 1 liquefaction PI 10329
- a-amylase Spezyme Alpha PF from Genencor (previously known as GC358) is added to a first wheat starch slurry having a dry substance of 32 w/w% at 47°C, in a double jacketed tank.
- the pH is about 5,7.
- the temperature is raised from 47°C to 54°C and maintained during 2 hours and 20 minutes.
- a pre-liquefact is obtained having a soiubilisation level of 12.5%.
- wheat starch (88% dry substance) is added gradually to obtain a second starch slurry having a dry substance of 51.6 w/w%.
- 0.03 w/w% a-amylase Spezyme Alpha PF and 0.034% a- amylase Liquozyme Supra 2.8X are also added gradually. This addition step is done in 30 minutes. The temperature is maintained during the whole time at 54°C. The solubilisation level of the second starch slurry is measured at 19.5%.
- the second starch slurry is leaving the tank at a rate of 1301/h.
- 90kg/h of dry wheat starch (88% dry substance) and 731/h of water is added to the tank.
- the process is running in a continuous way by adding fresh starch, enzymes and discharge the second starch slurry into a liquefaction step and this at a dry substance higher than what can be reached with the conventional process.
- the second starch slurry leaving the tank has a temperature of 54°C and is brought to a jet cooker where the temperature is increased to 107°C by steam injection. It is then maintained at a temperature of 107°C during 0 minutes and subsequently, after atmospheric flash, the temperature is reduced to about 98°C.
- the DE of the liquefact is measured at about 12 and the dry substance is about 48 w/w%.
- Further liquefaction is achieved by collecting said liquefact during 60 minutes and holding during 60 minutes at 95°C to 98°C until a DE of 23.3 is obtained.
- the liquefact at this stage is starch negative and can be sent continuously to the further processing steps.
- 0.01 w/w% of a-amylase Spezyme Alpha PF and 0.01 w/w% Liquozyme Supra 2.8 X is added to a first wheat starch slurry having a dry substance of 44.7 w/w% at 35°C, in a double jacketed tank.
- the pH is about 5.6.
- the temperature is maintained at 35°C during 1 0 minutes.
- a pre-liquefact is obtained having a solubilisation level of 5.1%.
- the pre-liquefact is leaving the tank at a rate of 1301/h.
- a starch slurry of 45w/w% dry substance is added to the tank at a rate of 1301/h.
- the pre-liquefact leaving the tank has a temperature of 35°C and is sent continuously to a second tank.
- 0.0085% Liquozyme Supra 2.8 X based on dry substance is added to the second tank.
- the average retention time in the second tank is 20 minutes.
- This mixture is brought continuously to a jet cooker where the temperature is increased to 107°C by steam injection, it is then maintained at a temperature of 107°C during 10 minutes and subsequently, after atmospheric flash, the temperature is reduced to about 98°C.
- the DE of this liquefact is measured at about 4.9 and the dry substance is about 42.3w/w%.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Zoology (AREA)
- Wood Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Genetics & Genomics (AREA)
- Emergency Medicine (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Description
Claims
Priority Applications (9)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
LTEP13747944.0T LT2785746T (en) | 2012-08-09 | 2013-08-07 | Process for starch liquefaction |
EP13747944.0A EP2785746B1 (en) | 2012-08-09 | 2013-08-07 | Process for starch liquefaction |
JP2015526666A JP6293146B2 (en) | 2012-08-09 | 2013-08-07 | Method for starch liquefaction |
US14/370,329 US10174130B2 (en) | 2012-08-09 | 2013-08-07 | Process for starch liquefaction |
ES13747944.0T ES2609811T3 (en) | 2012-08-09 | 2013-08-07 | Starch liquefaction procedure |
RU2015107998A RU2654248C2 (en) | 2012-08-09 | 2013-08-07 | Process for starch liquefaction |
CN201380041602.5A CN104520333B (en) | 2012-08-09 | 2013-08-07 | Starch liquefaction process |
AU2013299703A AU2013299703B2 (en) | 2012-08-09 | 2013-08-07 | Process for starch liquefaction |
ZA2015/00794A ZA201500794B (en) | 2012-08-09 | 2015-02-03 | Process for starch liquefaction |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP12005775 | 2012-08-09 | ||
EP12005775.7 | 2012-08-09 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2014025872A1 true WO2014025872A1 (en) | 2014-02-13 |
Family
ID=46832167
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2013/053929 WO2014025872A1 (en) | 2012-08-09 | 2013-08-07 | Process for starch liquefaction |
Country Status (13)
Country | Link |
---|---|
US (1) | US10174130B2 (en) |
EP (1) | EP2785746B1 (en) |
JP (2) | JP6293146B2 (en) |
CN (1) | CN104520333B (en) |
AR (1) | AR092093A1 (en) |
AU (1) | AU2013299703B2 (en) |
ES (1) | ES2609811T3 (en) |
HU (1) | HUE031009T2 (en) |
LT (1) | LT2785746T (en) |
PL (1) | PL2785746T3 (en) |
RU (1) | RU2654248C2 (en) |
WO (1) | WO2014025872A1 (en) |
ZA (1) | ZA201500794B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105695323B (en) * | 2016-03-16 | 2018-11-02 | 内蒙古玉王生物科技有限公司 | Efficient oligosaccharide biological enzyme production technology and equipments |
CN109402195B (en) * | 2017-11-02 | 2019-10-18 | 吉林中粮生化有限公司 | A kind of method of continuous liquefaction high concentration starch |
CN111272705A (en) * | 2020-03-23 | 2020-06-12 | 潍坊森瑞特生物科技有限公司 | Quick detection method for dextrin solubility |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4235965A (en) | 1976-05-12 | 1980-11-25 | Cpc International Inc. | Starch hydrolysis at high dry substance |
WO1993009244A1 (en) * | 1991-10-31 | 1993-05-13 | Genencor International, Inc. | Liquefaction of dry milled starch grain slurries |
EP0806434A1 (en) | 1996-05-06 | 1997-11-12 | National Starch and Chemical Investment Holding Corporation | High solids, single phase process for preparing enzyme converted starches |
US6184002B1 (en) * | 1995-06-02 | 2001-02-06 | Genencor International, Inc. | Method for liquefying starch |
US20030134396A1 (en) * | 2001-12-19 | 2003-07-17 | Shetty Jayarama K. | Process for hydrolyzing starch without pH adjustment |
US20110178288A1 (en) * | 2004-10-22 | 2011-07-21 | Cargill, Incorporated | Process for the production of maltodextrins and maltodextrins |
Family Cites Families (23)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3849194A (en) | 1966-12-19 | 1974-11-19 | Cpc International Inc | Low d.e. starch conversion products |
GB1200817A (en) | 1967-03-13 | 1970-08-05 | Union Starch And Refining Comp | Starch liquefaction process |
US3853706A (en) | 1967-03-30 | 1974-12-10 | Cpc International Inc | Process for producing non-waxy starch hydrolysates |
US3819484A (en) | 1970-12-16 | 1974-06-25 | Hayashibara Ken | Process for preparing sucrose-starch sweetner free from reducing sugar |
JPS5437211B1 (en) * | 1970-12-16 | 1979-11-14 | ||
US4298400A (en) | 1971-01-18 | 1981-11-03 | Grain Processing Corporation | Low D.E. starch conversion products |
JPS5312984B2 (en) | 1972-06-15 | 1978-05-06 | ||
JPS5244379B2 (en) | 1972-07-05 | 1977-11-08 | ||
US4014743A (en) * | 1973-01-10 | 1977-03-29 | Penick & Ford, Limited | Method for continuous preparation of cooked thinned starch pastes |
US4062728A (en) | 1975-07-11 | 1977-12-13 | Amstar Corporation | Starch thinning process |
US3974034A (en) | 1975-09-12 | 1976-08-10 | Cpc International Inc. | Malto-dextrins of improved stability prepared by enzymatic hydrolysis of oxidized starch |
SE7908105L (en) | 1979-10-01 | 1981-04-02 | Alfa Laval Ab | PROCEDURE FOR PREPARING ETHANOL BY CONTINUOUS RAISING OF POLYSACCHARIDE CONTAINING |
US4335208A (en) | 1980-03-11 | 1982-06-15 | Novo Industri A/S | Saccharification of starch hydrolysates |
JPS5765199A (en) | 1980-10-11 | 1982-04-20 | Agency Of Ind Science & Technol | Liquefaction of starch |
CN1189189A (en) * | 1995-06-02 | 1998-07-29 | 金克克国际有限公司 | Method for liquefying starch |
JP3460898B2 (en) | 1995-11-28 | 2003-10-27 | 月桂冠株式会社 | Liquor production apparatus and method |
EP0904360B1 (en) | 1996-04-30 | 2013-07-31 | Novozymes A/S | alpha-AMYLASE MUTANTS |
SG65045A1 (en) | 1997-01-29 | 1999-05-25 | Toray Industries | A method for continuously producing a cyclic formal |
DK1002062T3 (en) | 1997-07-02 | 2006-09-11 | Novozymes As | Starch conversion process using heat stable isoamylases from sulfolobus |
WO2006028897A2 (en) * | 2004-09-01 | 2006-03-16 | Novozymes North America, Inc. | Liquefaction and saccharifaction processes |
CN101048078A (en) * | 2004-10-22 | 2007-10-03 | 卡吉尔公司 | Process for the production of maltodextrins, and maltodextrins |
US7915020B2 (en) * | 2007-06-01 | 2011-03-29 | Syngenta Participations Ag | Process for starch liquefaction and fermentation |
RU2421525C1 (en) * | 2010-05-24 | 2011-06-20 | Юрий Ахметович Рамазанов | Method for production of molasses of starch |
-
2013
- 2013-08-07 AU AU2013299703A patent/AU2013299703B2/en not_active Ceased
- 2013-08-07 HU HUE13747944A patent/HUE031009T2/en unknown
- 2013-08-07 PL PL13747944T patent/PL2785746T3/en unknown
- 2013-08-07 US US14/370,329 patent/US10174130B2/en active Active
- 2013-08-07 LT LTEP13747944.0T patent/LT2785746T/en unknown
- 2013-08-07 EP EP13747944.0A patent/EP2785746B1/en active Active
- 2013-08-07 RU RU2015107998A patent/RU2654248C2/en active
- 2013-08-07 ES ES13747944.0T patent/ES2609811T3/en active Active
- 2013-08-07 CN CN201380041602.5A patent/CN104520333B/en active Active
- 2013-08-07 JP JP2015526666A patent/JP6293146B2/en active Active
- 2013-08-07 WO PCT/US2013/053929 patent/WO2014025872A1/en active Application Filing
- 2013-08-09 AR ARP130102844A patent/AR092093A1/en active IP Right Grant
-
2015
- 2015-02-03 ZA ZA2015/00794A patent/ZA201500794B/en unknown
-
2017
- 2017-11-17 JP JP2017221425A patent/JP6702926B2/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4235965A (en) | 1976-05-12 | 1980-11-25 | Cpc International Inc. | Starch hydrolysis at high dry substance |
WO1993009244A1 (en) * | 1991-10-31 | 1993-05-13 | Genencor International, Inc. | Liquefaction of dry milled starch grain slurries |
US6184002B1 (en) * | 1995-06-02 | 2001-02-06 | Genencor International, Inc. | Method for liquefying starch |
EP0806434A1 (en) | 1996-05-06 | 1997-11-12 | National Starch and Chemical Investment Holding Corporation | High solids, single phase process for preparing enzyme converted starches |
US20030134396A1 (en) * | 2001-12-19 | 2003-07-17 | Shetty Jayarama K. | Process for hydrolyzing starch without pH adjustment |
US20110178288A1 (en) * | 2004-10-22 | 2011-07-21 | Cargill, Incorporated | Process for the production of maltodextrins and maltodextrins |
Also Published As
Publication number | Publication date |
---|---|
ZA201500794B (en) | 2016-01-27 |
US20150166684A1 (en) | 2015-06-18 |
LT2785746T (en) | 2017-01-25 |
CN104520333A (en) | 2015-04-15 |
US10174130B2 (en) | 2019-01-08 |
EP2785746B1 (en) | 2016-10-12 |
AU2013299703B2 (en) | 2018-01-04 |
CN104520333B (en) | 2021-04-09 |
ES2609811T3 (en) | 2017-04-24 |
HUE031009T2 (en) | 2017-06-28 |
RU2015107998A (en) | 2016-09-27 |
JP6702926B2 (en) | 2020-06-03 |
RU2654248C2 (en) | 2018-05-17 |
EP2785746A1 (en) | 2014-10-08 |
PL2785746T3 (en) | 2017-06-30 |
JP2018075010A (en) | 2018-05-17 |
JP2015525825A (en) | 2015-09-07 |
AU2013299703A1 (en) | 2015-03-05 |
AR092093A1 (en) | 2015-03-25 |
JP6293146B2 (en) | 2018-03-14 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Aiyer | Amylases and their applications | |
RU2315811C2 (en) | Method for starch treatment | |
US20150037844A1 (en) | Liquefaction and saccharification of granular starch at high concentration | |
EP2430176B1 (en) | Improved production of maltotetraose syrup using a pseudomonas saccharophila maltotetraohydrolase variant and a debranching enzyme | |
US20090142812A1 (en) | Method for producing high molecular weight reduced viscosity starch pastes | |
WO2006066582A1 (en) | Fermentation product processes | |
JP6702926B2 (en) | Method for starch liquefaction | |
CN102321704B (en) | Method for treating starchy raw material and method for preparing citric acid | |
US20150111259A1 (en) | Method for Making High Maltose Syrup | |
US3783100A (en) | Non-retrograded thinned hydrolyzates | |
US20150152458A1 (en) | Low temperature method for making high glucose syrup | |
WO2000012746A1 (en) | Improved enzyme thinned starches | |
US20240114944A1 (en) | Method for producing slowly digestible branched starch hydrolysates and uses thereof | |
EP3668902A1 (en) | Process for obtaining maltodextrin and maltodextrin | |
Uppalanchi | Effect of starch structures on the efficiency of enzyme hydrolysis | |
Soetaredjo | The Effect of Reagents and Iodine Concentration on Sago Starch Acetylation and in vitro Digestibility | |
Umerie et al. | Biosynthesis and Characterization of Glucose Syrup Derived from Manihot Dulcis TMS 4 (2) 1423 Starch |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 13747944 Country of ref document: EP Kind code of ref document: A1 |
|
REEP | Request for entry into the european phase |
Ref document number: 2013747944 Country of ref document: EP |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2013747944 Country of ref document: EP |
|
WWE | Wipo information: entry into national phase |
Ref document number: 14370329 Country of ref document: US |
|
ENP | Entry into the national phase |
Ref document number: 2015526666 Country of ref document: JP Kind code of ref document: A |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
ENP | Entry into the national phase |
Ref document number: 2013299703 Country of ref document: AU Date of ref document: 20130807 Kind code of ref document: A |
|
WWE | Wipo information: entry into national phase |
Ref document number: IDP00201501346 Country of ref document: ID |
|
ENP | Entry into the national phase |
Ref document number: 2015107998 Country of ref document: RU Kind code of ref document: A |